CN115124766A - Preparation method of coated red phosphorus flame retardant - Google Patents
Preparation method of coated red phosphorus flame retardant Download PDFInfo
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- CN115124766A CN115124766A CN202210795430.1A CN202210795430A CN115124766A CN 115124766 A CN115124766 A CN 115124766A CN 202210795430 A CN202210795430 A CN 202210795430A CN 115124766 A CN115124766 A CN 115124766A
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- red phosphorus
- flame retardant
- coated
- zinc
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000003063 flame retardant Substances 0.000 title claims abstract description 44
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims abstract description 25
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011701 zinc Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 21
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002775 capsule Substances 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 12
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000003751 zinc Chemical class 0.000 claims abstract description 9
- 239000011787 zinc oxide Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 238000003756 stirring Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000002861 polymer material Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 229920000877 Melamine resin Polymers 0.000 description 4
- 239000004640 Melamine resin Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- JBFYUZGYRGXSFL-UHFFFAOYSA-N imidazolide Chemical compound C1=C[N-]C=N1 JBFYUZGYRGXSFL-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention provides a preparation method of a coated red phosphorus flame retardant, which comprises the following steps: (1) dispersing red phosphorus and polyethylene glycol in water, adding cyanuric acid and zinc oxide, and reacting for 2-6 h; (2) adding soluble zinc salt and 2-methylimidazole, adding ethylenediamine, reacting for 5-20 h, and dehydrating and drying the precipitate to obtain the red phosphorus-coated flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials. The red phosphorus-coated flame retardant provided by the invention has the characteristics of high whiteness, good oxidation resistance and high flame retardant efficiency.
Description
Technical Field
The invention relates to the field of flame retardant materials, in particular to a preparation method of a red phosphorus-coated flame retardant.
Background
Compared with other halogen-free flame retardants, the red phosphorus flame retardant has the advantages of high flame retardant efficiency, small using amount and the like, and is widely applied to the fields of rubber, nylon, polyester, epoxy resin, polyurethane and the like. However, pure red phosphorus has the defects of easy moisture absorption, unstable property, poor compatibility with high polymer materials, easy coloring and the like. After the red phosphorus is coated, the stability is improved, and the compatibility with a high polymer material is better. In addition, after the purple red of the red phosphorus is covered by the capsule material, the prepared coated red phosphorus has relatively light color and can be used for processing light-colored high polymer material products. Therefore, the coated red phosphorus serving as a flame retardant is added into a high polymer material, so that the defect of direct use of the red phosphorus can be overcome, and a considerable or even better flame retardant effect can be achieved.
At present, the mature red phosphorus coated product in the market is melamine resin coated red phosphorus, which takes melamine resin as a capsule wall material, has the characteristics of good oxidation resistance, low moisture absorption rate and good compatibility with high polymer materials, and is widely applied to processing of nylon, PET, PP and the like (pandeming, university of China and south, doctor thesis, 2004). However, melamine resin is transparent polymer resin, has poor covering property on red phosphorus color, has dark color, and cannot be used for processing light-colored polymer material products. In addition, the patent reports that a red phosphorus flame retardant coated by a zeolite imidazolate framework material and a preparation method (CN 202011228743.6) thereof, and discovers that ZIF-8 can be uniformly coated on the surface of red phosphorus, and the prepared ZIF-8 coated red phosphorus has better whiteness, oxidation resistance and flame retardant property. However, compared with common inorganic coating materials such as melamine resin, aluminum hydroxide and the like, the raw material cost of the ZIF-8 is high, and the large-scale application of the ZIF-8 coated red phosphorus is influenced. Therefore, the research on the ZIF-8 and the cheap material to cooperatively coat the red phosphorus can reduce the production cost, further improve the whiteness and the flame retardant property of the red phosphorus-coated flame retardant, and still have important significance for expanding the application range of the red phosphorus flame retardant.
Disclosure of Invention
The invention aims to provide a preparation method of a coated red phosphorus flame retardant, and the coated red phosphorus flame retardant obtained by the method has the advantages of high whiteness, good oxidation resistance, high flame retardant efficiency, lower cost and the like.
The invention provides a preparation method of a red phosphorus-coated flame retardant, which comprises the following steps:
(1) dispersing red phosphorus and polyethylene glycol in water, adding cyanuric acid and zinc oxide, and reacting for 2-6 h;
(2) adding soluble zinc salt, 2-methylimidazole and ethylenediamine, reacting for 5-20 h, and dehydrating and drying the precipitate to obtain the red phosphorus-coated flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials.
Further, the mass ratio of the polyethylene glycol to the red phosphorus is 1-6: 100.
further, the reaction temperature is 70-100 ℃.
Further, the molar ratio of cyanuric acid to red phosphorus is 0.2-0.4: 1.
further, the molar ratio of cyanuric acid to zinc oxide is 2-2.3: 3.
further, the zinc salt is zinc acetate, zinc nitrate, zinc chloride or zinc sulfate.
Further, Zn is contained in the zinc salt 2+ The molar ratio of the red phosphorus to the red phosphorus is 0.1-0.2: 1.
further, Zn is contained in the zinc salt 2+ The molar ratio to 2-methylimidazole is 1: 3 to 6.
Further, the molar ratio of the ethylenediamine to the 2-methylimidazole is 1: 5 to 10.
The preparation method has simple process, the red phosphorus surface is coated by zinc cyanurate and then is self-assembled with a ZIF-8 shell layer on the outer layer, the coating is uniform, and the red phosphorus-coated flame retardant has better color covering performance, so that the prepared red phosphorus-coated flame retardant has the characteristics of high whiteness and good oxidation resistance, and can be applied to the processing of light-colored high polymer materials.
The zinc cyanurate is a flame retardant with good color covering property and low cost; ZIF-8 is a novel capsule wall material which can be continuously self-assembled on the surface of a solid, can be uniformly coated on the surface of the solid, and has better synergistic flame retardant property. The zinc cyanurate and the ZIF-8 are taken as composite capsule materials for coating red phosphorus, and the advantages of the zinc cyanurate and the ZIF-8 can be effectively combined, so that the whiteness and the flame retardant property of the prepared zinc cyanurate and ZIF-8 composite coated red phosphorus are superior to those of zinc cyanurate or ZIF-8 single coated red phosphorus. Zinc cyanurate and ZIF-8 are used as the composite capsule wall material for coating red phosphorus, and have good synergistic effect.
Detailed Description
The following provides a more detailed description of the present invention. The above and other objects, features and advantages of the present invention will be apparent to those skilled in the art from the detailed description of the present invention.
Example 1
Dispersing 17 g of red phosphorus and 0.51 g of polyethylene glycol in 500 mL of water, adding 21 g of cyanuric acid and 18.5 g of zinc oxide, and reacting for 3 hours at 85 ℃ with stirring; adding 15 g of zinc acetate, 26 g of 2-methylimidazole and 2.5 g of ethylenediamine, continuously stirring for reacting for 10 hours, and dehydrating and drying precipitates obtained by the reaction to obtain the red phosphorus-coated flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials, wherein the red phosphorus content is 26%.
Example 2
Dispersing 17 g of red phosphorus and 0.25 g of polyethylene glycol in 600 mL of water, adding 14.5 g of cyanuric acid and 11.5 g of zinc oxide, and reacting for 6 hours at 70 ℃ with stirring; and then adding 20.5 g of zinc nitrate, 52 g of 2-methylimidazole and 6.5 g of ethylenediamine, continuously stirring for reacting for 20 hours, dehydrating and drying the precipitate obtained by the reaction to obtain the coated red phosphorus flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials, wherein the red phosphorus content is 29%.
Example 3
Dispersing 17 g of red phosphorus and 0.9 g of polyethylene glycol in 700 mL of water, 28 g of cyanuric acid and 26 g of zinc oxide, and reacting for 2 hours at 95 ℃ with stirring; and adding 9 g of zinc sulfate, 15 g of 2-methylimidazole and 1.1 g of ethylenediamine, continuously stirring for reacting for 5 hours, dehydrating and drying the precipitate obtained by the reaction to obtain the red phosphorus-coated flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials, wherein the red phosphorus content is 23%.
Comparative example 1
Dispersing 17 g of red phosphorus and 0.51 g of polyethylene glycol in 500 mL of water, adding 30.5 g of cyanuric acid and 28.5 g of zinc oxide, stirring at 85 ℃ for reaction for 13 h, dehydrating and drying a precipitate obtained by the reaction to obtain the coated red phosphorus flame retardant taking zinc cyanurate as a single capsule wall material, wherein the content of red phosphorus is 26%.
Comparative example 2
Dispersing 17 g of red phosphorus and 0.17 g of polyethylene glycol in 500 mL of water, adding 51 g of zinc acetate, 92 g of 2-methylimidazole and 9 g of ethylenediamine, stirring at 85 ℃ for reaction for 13 h, dehydrating and drying a precipitate obtained by the reaction to obtain the coated red phosphorus flame retardant taking ZIF-8 as a single capsule wall material, wherein the content of red phosphorus is 26%.
Performance test experiments:
the coated red phosphorus flame retardant samples prepared in examples 1 to 3, comparative example 1 and comparative example 2 were subjected to the following tests:
and (3) whiteness testing: weighing 10.00 g of sample, tabletting, placing in a sample box, and testing on a digital display whiteness instrument, wherein the results are shown in table 1;
and (3) oxidation resistance test: respectively weighing 10.00 g of sample in a three-neck flask containing 200 ml of distilled water, boiling the solution for 1 hour, filtering, removing initial filtrate, adding 10.00 g of analytically pure sodium chloride into 100 ml of the filtrate, titrating oxyacid formed by oxidation in the filtrate by using a standard sodium hydroxide solution after dissolution, and expressing the oxidation resistance of oxyacid by the milligrams of sodium hydroxide consumed by each gram of red phosphorus, wherein the results are shown in table 1;
limiting oxygen index test: the test was carried out according to the method of GB/T2406.2-2009, and the addition amount of the coated red phosphorus flame retardant was 12%, and the results are shown in Table 1.
From the test results of examples 1-3 in table 1, it can be seen that the red phosphorus-coated flame retardant using zinc cyanurate and ZIF-8 as composite capsule wall materials has high whiteness and flame retardant efficiency, and good oxidation resistance. According to the test results of the example 1, the comparative example 1 and the comparative example 2, the flame retardant performance and the whiteness of the coated red phosphorus using zinc cyanurate and ZIF-8 as composite capsule wall materials are obviously better compared with the coated red phosphorus sample using zinc cyanurate or ZIF-8 as single capsule wall material under the condition of the same red phosphorus content. The results show that the zinc cyanurate and the ZIF-8 are taken as the composite capsule wall material for coating red phosphorus, the advantages of the zinc cyanurate and the ZIF-8 can be effectively combined, and the zinc cyanurate and the ZIF-8 have good synergistic effect.
It should be understood that although the present invention has been clearly illustrated by the foregoing examples, various changes and modifications may be made therein by those skilled in the art without departing from the spirit and scope of the invention, and it is intended to cover all such changes and modifications as fall within the scope of the appended claims.
Claims (9)
1. The preparation method of the coated red phosphorus flame retardant is characterized by comprising the following steps:
(1) dispersing red phosphorus and polyethylene glycol in water, adding cyanuric acid and zinc oxide, and reacting for 2-6 h;
(2) adding soluble zinc salt, 2-methylimidazole and ethylenediamine, reacting for 5-20 h, and dehydrating and drying precipitates to obtain the red phosphorus-coated flame retardant taking zinc cyanurate and ZIF-8 as composite capsule wall materials.
2. The preparation method of the coated red phosphorus flame retardant according to claim 1, wherein the mass ratio of the polyethylene glycol to the red phosphorus is 1-6: 100.
3. the preparation method of the coated red phosphorus flame retardant according to claim 1, wherein the reaction temperature is 70-100 ℃.
4. The method for preparing the coated red phosphorus flame retardant of claim 1, wherein the molar ratio of cyanuric acid to red phosphorus is 0.2-0.4: 1.
5. the preparation method of the coated red phosphorus flame retardant of claim 1, wherein the molar ratio of the cyanuric acid to the zinc oxide is 2-2.3: 3.
6. the method of claim 1, wherein the zinc salt is zinc acetate, zinc nitrate, zinc chloride or zinc sulfate.
7. The method of claim 1, wherein Zn is contained in the zinc salt 2+ The molar ratio of the red phosphorus to the red phosphorus is 0.1-0.2: 1.
8. the method of claim 1, wherein Zn is added to the zinc salt 2+ The molar ratio to 2-methylimidazole is 1: 3 to 6.
9. The method of claim 1, wherein the molar ratio of ethylenediamine to 2-methylimidazole is 1: 5 to 10.
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